CN104464994A - High-performance permanent magnet material and production method thereof - Google Patents
High-performance permanent magnet material and production method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 77
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000010936 titanium Substances 0.000 claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 23
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010941 cobalt Substances 0.000 claims abstract description 9
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims description 56
- 230000008018 melting Effects 0.000 claims description 53
- 238000000034 method Methods 0.000 claims description 39
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 31
- 229910045601 alloy Inorganic materials 0.000 claims description 30
- 239000000956 alloy Substances 0.000 claims description 30
- 238000005496 tempering Methods 0.000 claims description 29
- 239000004576 sand Substances 0.000 claims description 27
- 239000000696 magnetic material Substances 0.000 claims description 26
- 229910052799 carbon Inorganic materials 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 238000005266 casting Methods 0.000 claims description 22
- 239000010949 copper Substances 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 20
- 229910052802 copper Inorganic materials 0.000 claims description 17
- 229910052742 iron Inorganic materials 0.000 claims description 17
- 239000013078 crystal Substances 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 11
- 230000006698 induction Effects 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 239000005864 Sulphur Substances 0.000 claims description 9
- 239000004411 aluminium Substances 0.000 claims description 9
- 239000000428 dust Substances 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 description 28
- 229910017709 Ni Co Inorganic materials 0.000 description 17
- 229910003267 Ni-Co Inorganic materials 0.000 description 17
- 229910003262 Ni‐Co Inorganic materials 0.000 description 17
- 238000002360 preparation method Methods 0.000 description 17
- 229910000831 Steel Inorganic materials 0.000 description 13
- 229910000828 alnico Inorganic materials 0.000 description 13
- 239000010959 steel Substances 0.000 description 13
- 230000005389 magnetism Effects 0.000 description 12
- 238000000465 moulding Methods 0.000 description 12
- 230000003068 static effect Effects 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000013461 design Methods 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 238000000227 grinding Methods 0.000 description 10
- 239000011449 brick Substances 0.000 description 8
- 238000005520 cutting process Methods 0.000 description 8
- 238000009413 insulation Methods 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- 235000013495 cobalt Nutrition 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 238000011160 research Methods 0.000 description 7
- 229910001570 bauxite Inorganic materials 0.000 description 6
- 229910000278 bentonite Inorganic materials 0.000 description 6
- 239000000440 bentonite Substances 0.000 description 6
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 229910001004 magnetic alloy Inorganic materials 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 230000000704 physical effect Effects 0.000 description 6
- 238000010791 quenching Methods 0.000 description 6
- 230000000171 quenching effect Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- -1 aluminium nickel cobalt Chemical compound 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 230000007774 longterm Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
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- Hard Magnetic Materials (AREA)
Abstract
The invention provides a high-performance permanent magnet material and a production method thereof, and particularly provides a permanent magnet material. The permanent magnet material comprises, by total weight, 30-50% of cobalt, 6-10% of titanium, 12-16% of nickel and 6-10% of aluminum. The permanent magnet material has excellent physical and magnetic performance.
Description
Technical field
The present invention relates to permanent magnetic material preparation field, particularly, the invention provides a kind of Al-Ni-Co permanent magnet material and preparation method thereof.
Background technology
Al-Ni-Co permanent magnet material is as first generation permanent magnetism, though it is lower to compare NdFeB, SmCo permanent magnetic material magnetic property, but because having excellent temperature stability, time stability, serviceability temperature can reach more than 600 DEG C, its chemical stability is good simultaneously, corrosion-resistant not oxidizable, make it have not replaceable effect at military industry field, be particularly suitable for using in the weaponrys such as torpedo, guided missile, aircraft and the requirement of satellite equally accurate is high, stability requirement is good spacecraft.
Compare the second generation and third generation permanent magnetic material, Al-Ni-Co permanent magnet material remanent magnetism is suitable with it, but coercive force and magnetic energy product lower, make the development need being more and more difficult to meet advanced weaponry equipment.In recent years along with China's national defense industrial expansion, the engineering of development advanced weaponry equipment gets more and more, many Al-Ni-Co permanent magnet component requirements permanent magnets not only have higher temperature stability in these areas, also require that magnet has higher coercive force to keep out the interference performance of external magnetic field simultaneously, higher magnetic field can be provided.So propose application demand to high-coercive force high-performance alnico magnet.
To the research work of high-coercive force alnico magnet, just research work is started abroad after developing non-oriented aluminium nickel cobalt 8, domestic is inchoate in mid-nineties 90 in last century 17, recent two decades comes, because the development of rare earth permanent-magnetic material neodymium iron boron is swift and violent, most of scientific research institutions and research institution all start the research turning to rare earth permanent-magnetic material, and the research work of aluminium nickel cobalt is carried out less, table 1 be according to current both at home and abroad report level of researching and producing compare, but general magnetic property is on the low side, be also difficult to the application demand meeting advanced weaponry equipment.
The domestic and international high-coercive force aluminium nickel cobalt of table 1 is researched and produced level and is compared
Cast aluminum-molykote composite material nickel cobalt can be divided into orientation aluminium nickel cobalt and non-oriented aluminium nickel cobalt according to its preparation technology.Obtain excellent magnetic energy product, the oriented crystalline structure that alnico alloy microstructure must have and the dual structure of magnetic anisotropy structure.For making alloy obtain higher coercive force, need the corresponding content increasing Co, Ti and Al.But, the increase of Al content can cause the fragility of material to increase, the increase of Ti then can the crystal grain of refiner material, along with the increase of Ti content, the difficulty obtaining columanar structure also increases, the difficulty obtaining high energy product increases relatively, particularly when Ti content is greater than 8% (mass fraction), still can not obtain the foundry goods of better column crystal under current industrial process conditions.The magnet steel for this reason simultaneously obtaining high-coercive force and high magnetic energy is a difficult problem in process of production.
In sum, this area still lacks one and has high-coercive force, also has both good physical property and the permanent magnetic material of magnetic property simultaneously.
Summary of the invention
The object of this invention is to provide one and there is high-coercive force, also have both good physical property and the permanent magnetic material of magnetic property simultaneously.
A first aspect of the present invention, provides a kind of permanent magnetic material, and described permanent magnetic material is the alloy comprising following component: cobalt, titanium, aluminium, and nickel; And
By the total weight of material, the content of described cobalt is 30 ~ 50wt%;
The content of described titanium is 6 ~ 10wt%;
The content of described nickel is 12 ~ 16wt%;
The content of described aluminium is 6 ~ 10wt%.
In another preference, described material also comprises the component being selected from lower group: copper, silicon, sulphur, iron, carbon, or its combination.
In another preference, described material also comprises silicon, carbon, or its combination.
In another preference, in described material, silicone content is 0.2 ~ 0.4wt% (preferably 0.2-0.3wt%); And/or carbon content is 0.05 ~ 0.20wt% (preferably 0.05-0.10wt%).
In another preference, in described material, the total weight by material:
The content of described copper is 2.5 ~ 4wt% (preferably 3-4wt%);
The content of described silicon is 0.2 ~ 0.4wt% (preferably 0.2-0.3wt%);
The content of described sulphur is 0.2 ~ 0.9wt%;
The content of described carbon is 0.07 ~ 0.1wt%;
The content of described iron is surplus, is preferably 8 ~ 43wt%.
In another preference, in described material, the total weight by material:
The content of described copper is 3 ~ 4wt%;
The content of described silicon is 0.2 ~ 0.25wt%;
The content of described iron is 8 ~ 43wt%;
The content of described sulphur is 0.4 ~ 0.9wt%;
The content of described carbon is 0.07 ~ 0.08wt%.
In another preference, in the material, by the total weight of material:
The content of described cobalt is 38 ~ 44wt%;
The content of described titanium is 7.5 ~ 8.4wt%;
The content of described nickel is 13.5 ~ 14.5wt%;
The content of described aluminium is 7.8 ~ 8.6wt%;
The content of described copper is 3 ~ 4wt%;
The content of described silicon is 0.2 ~ 0.25wt%;
The content of described sulphur is 0.4 ~ 0.9wt%;
The content of described iron is 19.2 ~ 29.6wt%; And
The content of described carbon is 0.07 ~ 0.08wt%.
In another preference, described material has one or more feature being selected from lower group:
Described material is columnar crystal structure; And/or
Described material crystalline orientation height is >=10-110mm; And/or
Described material residues magnetic induction density B r is 6.0-15kGs; Be preferably 8.0-10.5kGs; And/or
Described material coercivity H b is 1500Oe-3000Oe; Be preferably 1800Oe-2100Oe; And/or
Described material magnetic energy product (BH) m is 5.0-15.0MGOe; Be preferably 9.0-11.5MGOe.
A second aspect of the present invention, provide a kind of method for making of material as described in the first aspect of the invention, described method comprises step:
(1) melting is carried out to the mixture of each component, obtain melting mixture;
(2) described melting mixture is poured in sand mo(u)ld, obtains crystalline orientation alloy, and carry out solution treatment;
(3) the described alloy through solution treatment is placed in magnetic field to cool;
(4) magnetic field Isothermal treatment is carried out to described cooled alloy, obtain described material.
In another preference, before cast, first described sand mo(u)ld is positioned in baking oven and toasts.
In another preference, described baking temperature is 1200-1600 DEG C, is preferably 1300-1500 DEG C.
In another preference, described baking time is 5-60min, is preferably 10-30min.
In another preference, in described cast step, the temperature of described melting mixture controls at 1600-1700 DEG C, is preferably 1630-1670 DEG C.
In another preference, described solution treatment comprises: be fixed in sample box by described alloy, is positioned over a period of time in high temperature furnace.
In another preference, the temperature of described high temperature furnace is 1210 DEG C ~ 1250 DEG C.
In another preference, the time of described solution treatment is 2-20 minute.
In another preference, the magnetic field intensity in the magnetic field in described step (3) is 3000-5000Oe.
In another preference, in described cooling step, the direction of orientation of described alloy parallels with magnetic direction.
In another preference, in described cooling step, be cooled to described alloy surface blackening.
In another preference, in described cooling step, the temperature being cooled to described alloy is≤800 DEG C.
In another preference, described method also comprises:
In melting step: after first high melting point component being melted, add carbon dust and react a period of time, then add low-melting component; And/or
After described casting complete, the alloy obtained is incubated a period of time, then carries out sand removal process after cast.
Preferably, described high melting point component is Co, Fe, Ni, Cu component.
In another preference, the granularity of described carbon dust is 10-90 μm.
In another preference, described carbon dust is evenly laid on the melting liquid surface of high melting point component.
In another preference, described melting liquid and described carbon dust reaction time are 15-45s.
In another preference, described alloy and sand mo(u)ld are together incubated.
In another preference, cover sand mo(u)ld with stay-warm case and be incubated.
In another preference, described temperature retention time is 0.5-6h.
In another preference, described Isothermal treatment step comprises:
Regulate the temperature of Isothermal treatment environment at 815-830 DEG C; And/or
Control the temperature difference≤± 1 DEG C of Isothermal treatment environment, be preferably≤± 0.5 DEG C; And/or;
The time of described Isothermal treatment is 5-30min, is preferably 10-25min.
In another preference, described method also comprises:
I () be pre-prepared sand mo(u)ld before described cast step;
(ii) after described Isothermal treatment step, temper is carried out to obtained material.
In another preference, after described cast step and before described solutionizing step, cutting processing is carried out to the alloy that described cast step obtains.
In another preference, described temper comprises step:
One-level tempering: be incubated 1-5 hour at 650 DEG C ~ 690 DEG C;
Second annealing: be incubated 6-10 hour at 600 DEG C ~ 640 DEG C;
Three grades of tempering: be incubated 12-24 hour at 550 DEG C ~ 590 DEG C.
In another preference, in described tempering step at different levels, every grade of cooling rate is 0.01-2 DEG C/min, is preferably 0.07 ~ 0.1 DEG C/min.
Should be understood that within the scope of the present invention, above-mentioned each technical characteristic of the present invention and can combining mutually between specifically described each technical characteristic in below (eg embodiment), thus form new or preferred technical scheme.As space is limited, tiredly no longer one by one to state at this.
Accompanying drawing explanation
The magnetic property curve chart of Fig. 1, embodiment 1 sample;
The magnetic property curve chart of Fig. 2, embodiment 2 sample;
The magnetic property curve chart of Fig. 3, embodiment 3 sample;
The magnetic property curve chart of Fig. 4, embodiment 4 sample;
The change curve of Fig. 5, embodiment 2 magnetic sample performance and one-level temperature;
Fig. 6, embodiment 2 foundry goods longitudinal section crystal morphology figure;
Fig. 7, comparative example ingot casting longitudinal section crystal morphology figure;
The magnetic property curve of Fig. 8, comparative example.
Embodiment
The present inventor, through long-term and deep research, has unexpectedly obtained a kind of permanent magnetic material with excellent properties.Described material both had high-coercive force, also had both good physical property and magnetic property simultaneously.Based on above-mentioned discovery, inventor completes the present invention.
Term
As used herein, term " permanent magnetic material " refers to the material that can keep constant magnetic once magnetization, and term " permanent-magnet alloy " refers to the permanent magnetic material of metal material.
Term " Al-Ni-Co permanent magnet ", " alnico " or " Al-Ni-Co permanent magnet material " refer to elements such as nickel, aluminium, cobalts for main component, the hold concurrently permanent magnetic material or permanent-magnet alloy that contain other elements.Preferably, Al-Ni-Co permanent magnet of the present invention is Al-Ni-Co permanent magnet of the present invention, has component as described in the first aspect of the invention.
Term " crystalline orientation " or " crystal orientation " refer to that metallic atom forms crystal orientation structure (asking inventor suitably to fill in) according to temperature gradient direction arrangement crystallisation by cooling in cooling procedure.In the present invention, crystalline orientation height is characterized by crystal length in the longitudinal section of observation by light microscope measurement foundry goods.
Al-Ni-Co permanent magnet
The present invention aims to provide a kind of Al-Ni-Co permanent magnet, and this magnet has high coercive force, the magnetic property simultaneously had and physical property.Particularly, permanent magnetic material provided by the invention is the alloy comprising following component: cobalt, titanium, aluminium, and nickel; And
By the total weight of material, the content of described cobalt is 30 ~ 50wt%;
The content of described titanium is 6 ~ 10wt%;
The content of described nickel is 12 ~ 16wt%;
The content of described aluminium is 6 ~ 10wt%.
Except above-mentioned key component, described material also comprises the component being selected from lower group: copper, silicon, sulphur, iron, carbon, or its combination.Other constituent contents except key component can be arbitrary proportions, as adjusted according to the character of material requested.
In another preference, described material also comprises silicon, carbon, or its combination.
In another preference, in described material, silicone content is 0.2 ~ 0.4wt% (preferably 0.2-0.3wt%); And/or carbon content is 0.05 ~ 0.20wt% (preferably 0.05-0.10wt%).
In a preference of the present invention, in described material, the total weight by material:
The content of described copper is 2.5 ~ 4wt% (preferably 3-4wt%);
The content of described silicon is 0.2 ~ 0.4wt% (preferably 0.2-0.3wt%);
The content of described sulphur is 0.2 ~ 0.9wt%;
The content of described carbon is 0.07 ~ 0.1wt%;
The content of described iron is surplus, is preferably 8 ~ 43wt%.
In described material, each element can exist with arbitrary form, as simple substance and compound.
In another preference, in the material, by the total weight of material:
The content of described cobalt is 38 ~ 44wt%; And/or
The content of described titanium is 7.5 ~ 8.4wt%; And/or
The content of described nickel is 13.5 ~ 14.5wt%; And/or
The content of described aluminium is 7.8 ~ 8.6wt%; And/or
The content of described copper is 3 ~ 4wt%; And/or
The content of described silicon is 0.2 ~ 0.25wt%; And/or
The content of described sulphur is 0.4 ~ 0.9wt%; And/or
The content of described iron is 19.2 ~ 29.6wt%; And/or
The content of described carbon is 0.07 ~ 0.08wt%.
Described material has high coercive force, the magnetic property simultaneously had and physical property.In a preference of the present invention, described material has one or more physical parameter being selected from lower group:
Crystalline orientation height is 10-110; And/or
Residual induction intensity Br is 6.0-15kGs; Be preferably 8.0-10.5kGs; And/or
Coercivity H b is 1500Oe-3000Oe; Be preferably 1800Oe-2100Oe; And/or
Magnetic energy product (BH) m is 5.0-15.0MGOe; Be preferably 9.0-11.5MGOe.
The preparation of Al-Ni-Co permanent magnet
Present invention also offers the method for making of above-mentioned material, described method comprises step:
(1) melting is carried out to the mixture of each component, obtain melting mixture;
(2) pour into a mould with described melting mixture, obtain crystalline orientation alloy, and carry out solution treatment;
(3) the described molten alloy through solution treatment is placed in magnetic field to cool;
(4) magnetic field Isothermal treatment is carried out to described cooled molten alloy, obtain described material.
In another preference, in described cast step, the temperature of described melting mixture controls at 1600-1700 DEG C, is preferably 1630-1670 DEG C.
For obtaining the better material of performance, described melting mixture need be placed in magnetic field and cool.Preferably, in described cooling step, the direction of orientation of described melting mixture parallels with magnetic direction.
In another preference, in described cooling step, be cooled to described molten alloy surface stain.
In another preference, in described cooling step, the temperature being cooled to described molten alloy is≤800 DEG C.
In another preference, described melting step comprises: after first being melted by high melting point component, adds carbon dust and reacts a period of time, then add low-melting component.Preferably, described high melting point component is Co, Fe, Ni, Cu component.In another preference, the granularity of described carbon dust is 10-90 μm.
In another preference, described carbon dust is evenly laid on the melting liquid surface of high melting point component.
In another preference, described melting liquid and described carbon dust reaction time are 15-45s.
Wherein, preferred Isothermal treatment step also comprises:
Regulate the temperature of Isothermal treatment environment at 815-830 DEG C; And/or
Control the temperature difference≤± 1 DEG C of Isothermal treatment environment, be preferably≤± 0.5 DEG C; And/or;
The time of described Isothermal treatment is 5-30min, is preferably 10-25min.
In another preference, the magnetic field intensity in the magnetic field of described Isothermal treatment is 3000-5000Oe.
In another preference, described method also comprises:
I () be pre-prepared sand mo(u)ld before described cast step;
(ii) after described cast step and before described solutionizing step, cutting processing is carried out to the melting mixture after described cast;
(iii) after described Isothermal treatment step, temper is carried out to obtained material.
Preferably, described method also comprises, and after described casting complete, is incubated by the melting mixture after cast.Preferred incubation step comprises: at the bottom of sand mo(u)ld and sand mo(u)ld, brick is together placed in baking oven and toasts, and after molten steel is poured into sand mo(u)ld completely, covers dead head rapidly with brick at the bottom of sand mo(u)ld, and stay-warm case is covered whole sand mo(u)ld and be incubated.
In another preference, described temperature retention time is 0.5-6h.
In a preferred embodiment of the invention, described temper comprises step:
One-level tempering: be incubated 1-5 hour at 650 DEG C ~ 690 DEG C;
Second annealing: be incubated 6-10 hour at 600 DEG C ~ 640 DEG C;
Three grades of tempering: be incubated 12-24 hour at 550 DEG C ~ 590 DEG C.
In another preference, after described three grades of tempering steps, take out after cooling to described material with the furnace room temperature.Preferably, in described tempering step at different levels, every grade of cooling rate is 0.01-2 DEG C/min, is preferably 0.07 ~ 0.1 DEG C/min.
A kind of preferred preparation method carries out according to the following steps:
(1) moulding: the bauxite mixing adopting different-grain diameter, adds bentonite and appropriate water makees binding agent, mixes rear static placement and starts moulding after 24 hours.Sand mo(u)ld comprises honeycomb fashion casting mold and dead head two parts of a mould eight.
(2) melting and cast: adopt medium frequency induction melting furnace melting, first by after Co, Ni, Fe, Cu tetra-kinds of high-melting-point elements melt during melting, the C powder adding granularity about tens μm makes it be layered on molten steel surface uniformly, react about 30 seconds, Si, FeS, Ti, Al are added in molten steel, stir, pour into a mould after static 3 minutes, pouring temperature controls at 1650 DEG C ± about 20 DEG C.Sand mo(u)ld takes out to be placed on water mold fast after 20 minutes through 1400 DEG C of bakings and pours into a mould in baking mill stove.Cover dead head with brick at the bottom of same mould after overbaking after casting complete, cover casting mold with stay-warm case fast and be incubated half an hour more than, sand removal process after cooling completely.
(3) cutting processing: go out required size with linear cutter by after the cast(ing) surface shakeout cleaned out.
(4) solution treatment: by the product of machine-shaping, is fixed in sample box and is placed in high temperature furnace 1210 DEG C ~ 1250 DEG C solution treatment 10 minutes.
(5) cool in magnetic field: from Solution Treatment Furnace, take out sample box, be placed on rapidly in the magnetic field of about 3500Oe, ensure that sample direction of orientation parallel magnetic field direction is placed, use air blast quenching, be cooled to sample surfaces blackening (less than 800 DEG C) and put isothermal processes to magnetic heat treatment furnace fast.
(6) magnetic field Isothermal treatment: magnetic field: 3500Oe ~ 4500Oe, isothermal temperature 815 ~ 830 DEG C, isothermal time 12min ~ 22min, ensure that parallel magnetic field direction, sample grain orientation direction is placed, accurate control electric furnace programming rate and temperature-controlled precision, make to rise to design temperature in 4 ~ 6 minutes, holding temperature controls within ± 0.5 DEG C.
(7) temper: adopt three grades of tempering process, between every grade, cooling rate controls within 0.07 ~ 0.1 DEG C/min.One-level tempering: 650 DEG C ~ 690 DEG C are incubated 3 hours; Second annealing 600 DEG C ~ 640 DEG C insulation 8 hours; Take out after three grades of tempering, 550 DEG C ~ 590 DEG C insulations cooled to room temperature with the furnace after 16 hours.
Major advantage of the present invention:
1, permanent magnetic material of the present invention has straight and upright thick columnar crystal structure, and crystalline orientation height reaches more than 80mm, compensate for the blank of prior art.
2, permanent magnetic material provided by the invention has excellent performance, is particularly maintaining beyond good physical properties and magnetic property, also has good crystalline orientation and very outstanding coercive force character and magnetic energy product character, applied range.
3, preparation method provided by the present invention can prepare and have excellent crystal structure, and magnetic structure is good, the permanent magnetic material of mechanical performance and chemical property excellence.Production technology is easy, low for equipment requirements, is suitable for very much industrial mass production permanent magnetic material.
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.The experimental technique of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.Unless otherwise indicated, otherwise percentage and number calculate by weight.
Embodiment 1
A kind of high-coercive force high-performance aluminum Ni-Co permanent magnetic alloy presses Al:8.6%; Ni:14.5%; Co:44.0%; Cu:4.0%; Ti:8.4%; C:0.08%; FeS:1.1%; Si:0.25%; Fe is surplus design composition, is prepared after preparation raw material.
A preparation technology for high-coercive force high-performance aluminum Ni-Co permanent magnetic alloy, carries out according to the following steps:
(1) moulding: the bauxite mixing adopting different-grain diameter, adds bentonite and appropriate water makees binding agent, mixes rear static placement and starts moulding after 24 hours.Sand mo(u)ld comprises honeycomb fashion casting mold and dead head two parts of a mould eight.
(2) melting and cast: adopt medium frequency induction melting furnace melting, first by after Co, Ni, Fe, Cu tetra-kinds of high-melting-point elements melt during melting, the C powder adding granularity about tens μm makes it be layered on molten steel surface uniformly, react about 30 seconds, Si, FeS, Ti, Al are added in molten steel, stir, pour into a mould after static 3 minutes, pouring temperature controls at 1650 DEG C ± about 20 DEG C.Sand mo(u)ld takes out to be placed on water mold fast after 20 minutes through 1400 DEG C of bakings and pours into a mould in baking mill stove.Cover dead head with brick at the bottom of same mould after overbaking after casting complete, cover casting mold with stay-warm case fast and be incubated half an hour more than, sand removal process after cooling completely.
(3) cutting processing: will the cylinder of linear cutter size ￠ 10*35mm be used after the cast(ing) surface shakeout cleaned out stand-by.
(4) solution treatment: the cylinder getting three ￠ 10*35mm at random, is fixed in sample box and is placed in preheating furnace after 800 DEG C of preheatings, to be placed in high temperature furnace 1210 DEG C of solution treatment 10 minutes.
(5) magnetic-field cooling: take out sample box from Solution Treatment Furnace, be placed on rapidly in the magnetic field of about 3500Oe, ensure that sample direction of orientation parallel magnetic field direction is placed, use air blast quenching, be cooled to sample surfaces blackening (less than 800 DEG C) and put isothermal processes to magnetic heat treatment furnace fast.
(6) magnetic field Isothermal treatment: magnetic field is 4000Oe, isothermal temperature 819 DEG C, isothermal time 18min, accurately control electric furnace programming rate and temperature-controlled precision, make to rise to design temperature in 4 ~ 6 minutes, holding temperature controls within ± 0.5 DEG C.
(7) temper: adopt two-stage tempering process, between every grade, cooling rate controls within 0.1 DEG C/min.One-level tempering: 692 DEG C insulation 3 hours after at a slow speed (0.07 DEG C/min) be down to 590 DEG C insulation 6 hours after cool to room temperature with the furnace.
(8) fine grinding detects: adopt centreless grinding and plane to grind off except product surface oxide skin, the NIM500C permanent magnetic material measuring instrument that china institute of metrology is produced detects magnetic property according to GB GB-T3217-1992 permanent magnetism (Hard Magnetic) magnetism of material experimental technique, and test magnetic property is in table 2.
Sample size: Φ 10*35mm, testing environment temperature is 20 DEG C, and the magnetic property curve chart of sample as shown in Figure 1.
Embodiment 2
A kind of high-coercive force high-performance aluminum Ni-Co permanent magnetic alloy presses Al:8.4%; Ni:14%; Co:40.0%; Cu:3.0%; Ti:8.2%; C:0.08%; FeS:1.1%; Si:0.25%; Fe is surplus design composition, is prepared after preparation raw material.
A preparation method for high-coercive force high-performance aluminum Ni-Co permanent magnetic alloy, carries out according to the following steps:
(1) moulding: the bauxite mixing adopting different-grain diameter, adds bentonite and appropriate water makees binding agent, mixes rear static placement and starts moulding after 24 hours.Sand mo(u)ld comprises honeycomb fashion casting mold and dead head two parts of a mould eight.
(2) melting and cast: adopt medium frequency induction melting furnace melting, first by after Co, Ni, Fe, Cu tetra-kinds of high-melting-point elements melt during melting, the C powder adding granularity about tens μm makes it be layered on molten steel surface uniformly, react about 30 seconds, Si, FeS, Ti, Al are added in molten steel, stir, pour into a mould after static 3 minutes, pouring temperature controls at 1650 DEG C ± about 20 DEG C.Sand mo(u)ld takes out to be placed on water mold fast after 20 minutes through 1400 DEG C of bakings and pours into a mould in baking mill stove.Cover dead head with brick at the bottom of same mould after overbaking after casting complete, cover casting mold with stay-warm case fast and be incubated half an hour more than, sand removal process after cooling completely.The longitudinal section crystal morphology of gained foundry goods as shown in Figure 6.
(3) cutting processing: will the cylinder of linear cutter size ￠ 10*35mm be used after the cast(ing) surface shakeout cleaned out stand-by.
(4) solution treatment: the cylinder getting three ￠ 10*35mm at random, is fixed in sample box and is placed in preheating furnace after 800 DEG C of preheatings, to be placed in high temperature furnace 1220 DEG C of solution treatment 10 minutes.
(5) magnetic-field cooling: take out sample box from Solution Treatment Furnace, be placed on rapidly in the magnetic field of about 3500Oe, ensure that sample direction of orientation parallel magnetic field direction is placed, use air blast quenching, be cooled to sample surfaces blackening (less than 800 DEG C) and put isothermal processes to magnetic heat treatment furnace fast.
(6) magnetic field Isothermal treatment: magnetic field is 4000Oe, isothermal temperature 819 DEG C, isothermal time 20min, ensure that parallel magnetic field direction, sample grain orientation direction is placed, accurate control electric furnace programming rate and temperature-controlled precision, make to rise to design temperature in 4 ~ 6 minutes, holding temperature controls within ± 0.5 DEG C.
(7) temper: adopt three grades of tempering process, between every grade, cooling rate controls within 0.1 DEG C/min.One-level tempering: 690 DEG C are incubated 3 hours; Second annealing: 640 DEG C are incubated 8 hours; Three grades of tempering: 590 DEG C of insulations cooled to room temperature with the furnace after 16 hours.
(8) fine grinding detects: adopt centreless grinding and plane to grind off except product surface oxide skin, the NIM500C permanent magnetic material measuring instrument that china institute of metrology is produced detects magnetic property according to GB GB-T3217-1992 permanent magnetism (Hard Magnetic) magnetism of material experimental technique, and test magnetic property is in table 2.
Magnetic property curve detection condition: sample size: Φ 10*35mm, testing environment temperature is 20 DEG C; Magnetic property is with the experiment condition of one-level temperature change curve: same Φ 10*35mm sample changes one-level temperature from low to high, every tempering is put into tempering furnace after once taking out afterwards and detecting agnetic property at room temperature m and is adjusted the tempering again of one-level temperature, by that analogy, the situation of change increasing magnetic property with one-level temperature is contrasted.
The magnetic property curve chart of sample as shown in Figure 2, magnetic sample performance with the change curve of one-level temperature as shown in Fig. 5 A, 5B, 5C, 5D.
Embodiment 3
A kind of high-coercive force high-performance aluminum Ni-Co permanent magnetic alloy presses Al:7.8%; Ni:13.5%; Co:40.0%; Cu:3.0%; Ti:7.5%; C:0.08%; FeS:1.1%; Si:0.25%; Fe is surplus design composition, is prepared after preparation raw material.
A preparation method for high-coercive force high-performance aluminum Ni-Co permanent magnetic alloy, carries out according to the following steps:
(1) moulding: the bauxite mixing adopting different-grain diameter, adds bentonite and appropriate water makees binding agent, mixes rear static placement and starts moulding after 24 hours.Sand mo(u)ld comprises honeycomb fashion casting mold and dead head two parts of a mould eight.
(2) melting and cast: adopt medium frequency induction melting furnace melting, first by after Co, Ni, Fe, Cu tetra-kinds of high-melting-point elements melt during melting, the C powder adding granularity about tens μm makes it be layered on molten steel surface uniformly, react about 30 seconds, Si, FeS, Ti, Al are added in molten steel, stir, pour into a mould after static 3 minutes, pouring temperature controls at 1650 DEG C ± about 20 DEG C.Sand mo(u)ld takes out to be placed on water mold fast after 20 minutes through 1400 DEG C of bakings and pours into a mould in baking mill stove.Cover dead head with brick at the bottom of same mould after overbaking after casting complete, cover casting mold with stay-warm case fast and be incubated half an hour more than, sand removal process after cooling completely.
(3) cutting processing: will the cylinder of linear cutter size ￠ 10*35mm be used after the cast(ing) surface shakeout cleaned out stand-by.
(4) solution treatment: the cylinder getting three ￠ 10*35mm at random, is fixed in sample box and is placed in preheating furnace after 800 DEG C of preheatings, to be placed in high temperature furnace 1220 DEG C of solution treatment 10 minutes.
(5) magnetic-field cooling: take out sample box from Solution Treatment Furnace, be placed on rapidly in the magnetic field of about 3500Oe, ensure that sample direction of orientation parallel magnetic field direction is placed, use air blast quenching, be cooled to sample surfaces blackening (less than 800 DEG C) and put isothermal processes to magnetic heat treatment furnace fast.
(6) magnetic field Isothermal treatment: magnetic field is 4000Oe, isothermal temperature 819 DEG C, isothermal time 20min, ensure that parallel magnetic field direction, sample grain orientation direction is placed, accurate control electric furnace programming rate and temperature-controlled precision, make to rise to design temperature in 4 ~ 6 minutes, holding temperature controls within ± 0.5 DEG C.
(7) temper: adopt three grades of tempering process, between every grade, cooling rate controls within 0.1 DEG C/min.One-level tempering: 660 DEG C are incubated 3 hours; Second annealing: 610 DEG C are incubated 8 hours; Three grades of tempering: 560 DEG C of insulations cooled to room temperature with the furnace after 16 hours.
(8) fine grinding detects: adopt centreless grinding and plane to grind off except product surface oxide skin, on the NIM500C permanent magnetic material measuring instrument that china institute of metrology is produced, detect magnetic property according to GB GB-T3217-1992 permanent magnetism (Hard Magnetic) magnetism of material experimental technique, test result is in table 2.
Testing conditions is with embodiment 1, and the magnetic property curve chart of sample as shown in Figure 3.
Embodiment 4
Al:7.8% pressed by a kind of high-coercive force alnico; Ni:13.5%; Co:38.0%; Cu:3.0%; Ti:7.5%; C:0.08%; FeS:1.1%; Si:0.20%; Fe is surplus design composition, is prepared after preparation raw material.
A preparation technology for high-coercive force alnico, carries out according to the following steps:
(1) moulding: the bauxite mixing adopting different-grain diameter, adds bentonite and appropriate water makees binding agent, mixes rear static placement and starts moulding after 24 hours.Sand mo(u)ld comprises honeycomb fashion casting mold and dead head two parts of a mould eight.
(2) melting and cast: adopt medium frequency induction melting furnace melting, first by after Co, Ni, Fe, Cu tetra-kinds of high-melting-point elements melt during melting, the C powder adding granularity about tens μm makes it be layered on molten steel surface uniformly, react about 30 seconds, Si, FeS, Ti, Al are added in molten steel, stir, pour into a mould after static 3 minutes, pouring temperature controls at 1650 DEG C ± about 20 DEG C.Sand mo(u)ld takes out to be placed on water mold fast after 20 minutes through 1400 DEG C of bakings and pours into a mould in baking mill stove.Cover dead head with brick at the bottom of same mould after overbaking after casting complete, cover casting mold with stay-warm case fast and be incubated half an hour more than, sand removal process after cooling completely.
(3) cutting processing: will the cylinder of linear cutter size ￠ 10*35mm be used after the cast(ing) surface shakeout cleaned out stand-by.
(4) solution treatment: the cylinder getting three ￠ 10*35mm at random, is fixed in sample box and is placed in preheating furnace after 800 DEG C of preheatings, to be placed in high temperature furnace 1220 DEG C of solution treatment 10 minutes.
(5) magnetic-field cooling: take out from Solution Treatment Furnace in the magnetic field being placed on rapidly 3500Oe and use air blast quenching, is cooled to surface stain (less than 800 DEG C) and puts isothermal processes to magnetic heat treatment furnace fast.
(6) magnetic field Isothermal treatment: magnetic field is 4000Oe, isothermal temperature 819 DEG C, isothermal time 15min, ensure that parallel magnetic field direction, sample grain orientation direction is placed, accurate control electric furnace programming rate and temperature-controlled precision, make to rise to design temperature in 4 ~ 6 minutes, holding temperature controls within ± 0.5 DEG C.
(7) temper: adopt three grades of tempering process, between every grade, cooling rate controls within 0.1 DEG C/min.One-level tempering: 655 DEG C are incubated 3 hours; Second annealing: 605 DEG C are incubated 8 hours; Three grades of tempering: 555 DEG C of insulations cooled to room temperature with the furnace after 16 hours.
(8) fine grinding detects: adopt centreless grinding and plane to grind off except product surface oxide skin, on the NIM500C permanent magnetic material measuring instrument that china institute of metrology is produced, detect magnetic property according to GB GB-T3217-1992 permanent magnetism (Hard Magnetic) magnetism of material experimental technique, test result is in table 2.
Testing conditions is with embodiment 1, and the magnetic property curve chart of sample as shown in Figure 4.
Comparative example
Al:8.4% pressed by a kind of high-coercive force alnico; Ni:14%; Co:40.0%; Cu:3.0%; Ti:8.2%; C: do not add; FeS:1.1%; Si: do not add; Fe is surplus design composition, is prepared after preparation raw material.
A preparation technology for high-coercive force alnico, carries out according to the following steps:
(1) moulding: the bauxite mixing adopting different-grain diameter, adds bentonite and appropriate water makees binding agent, mixes rear static placement and starts moulding after 24 hours.Sand mo(u)ld comprises honeycomb fashion casting mold and dead head two parts of a mould eight.
(2) melting and cast: adopt medium frequency induction melting furnace melting, first by after Co, Ni, Fe, Cu tetra-kinds of high-melting-point elements melt during melting, FeS, Ti, Al are added in molten steel, stir, pour into a mould after static 3 minutes, pouring temperature controls at 1650 DEG C ± about 20 DEG C.Sand mo(u)ld takes out to be placed on water mold fast after 20 minutes through 1400 DEG C of bakings and pours into a mould in baking mill stove.Cover dead head with brick at the bottom of same mould after overbaking after casting complete, cover casting mold with stay-warm case fast and be incubated half an hour more than, sand removal process after cooling completely.In the longitudinal section of gained foundry goods, crystal morphology as shown in Figure 7.
(3) cutting processing: will the cylinder of linear cutter size ￠ 10*35mm be used after the cast(ing) surface shakeout cleaned out stand-by.
(4) solution treatment: the cylinder getting three ￠ 10*35mm at random, is fixed in sample box and is placed in preheating furnace after 800 DEG C of preheatings, to be placed in high temperature furnace 1220 DEG C of solution treatment 10 minutes.
(5) magnetic-field cooling: take out from Solution Treatment Furnace in the magnetic field being placed on rapidly 3500Oe and use air blast quenching, is cooled to surface stain (less than 800 DEG C) and puts isothermal processes to magnetic heat treatment furnace fast.
(6) magnetic field Isothermal treatment: magnetic field is 4000Oe, isothermal temperature 819 DEG C, isothermal time 15min, accurately control electric furnace programming rate and temperature-controlled precision, make to rise to design temperature in 4 ~ 6 minutes, holding temperature controls within ± 0.5 DEG C.
(7) temper: adopt three grades of tempering process, between every grade, cooling rate controls within 0.1 DEG C/min.One-level tempering: 655 DEG C are incubated 3 hours; Second annealing: 605 DEG C are incubated 8 hours; Three grades of tempering: 555 DEG C of insulations cooled to room temperature with the furnace after 16 hours.
(8) fine grinding detects: adopt centreless grinding and plane to grind off except product surface oxide skin, on the NIM500C permanent magnetic material measuring instrument that china institute of metrology is produced, detect magnetic property according to GB GB-T3217-1992 permanent magnetism (Hard Magnetic) magnetism of material experimental technique, test result is in table 2.
Testing conditions: sample test direction is identical with process direction, magnetic field, other conditions are with embodiment 1, and the magnetic property curve chart of sample as shown in Figure 8.
Result shows, and the alloy not adding C, Si component fails to be formed the columnar crystal structure of alloy in embodiment 1-4, and compares the alloy of embodiment 1-4, and the alloy not adding C, Si component shows poor magnetic property.
The list of table 2 product magnetic property
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after having read above-mentioned instruction content of the present invention.
Claims (10)
1. a permanent magnetic material, is characterized in that, described permanent magnetic material is the alloy comprising following component: cobalt, titanium, aluminium, and nickel; And
By the total weight of material, the content of described cobalt is 30 ~ 50wt%;
The content of described titanium is 6 ~ 10wt%;
The content of described nickel is 12 ~ 16wt%;
The content of described aluminium is 6 ~ 10wt%.
2. material as claimed in claim 1, it is characterized in that, described material also comprises the component being selected from lower group: copper, silicon, sulphur, iron, carbon, or its combination.
3. material as claimed in claim 2, is characterized in that, in described material, and the total weight by material:
The content of described copper is 2.5 ~ 4wt%;
The content of described silicon is 0.2 ~ 0.4wt%;
The content of described sulphur is 0.2 ~ 0.9wt%;
The content of described carbon is 0.07 ~ 0.1wt%;
The content of described iron is surplus, is preferably 8 ~ 43wt%.
4. material as claimed in claim 2, it is characterized in that, described material has one or more feature being selected from lower group:
Described material is columnar crystal structure; And/or
Described material crystalline orientation height is 10-110mm; And/or
Described material residues magnetic induction density B r is 6.0-15kGs; And/or
Described material coercivity H b is 1500Oe-3000Oe; And/or
Described material magnetic energy product (BH) m is 5.0-15.0MGOe.
5. material as claimed in claim 1, it is characterized in that, described material has one or more feature being selected from lower group:
Described material is columnar crystal structure; And/or
Described material crystalline orientation height is >=80mm; And/or
Described material residues magnetic induction density B r is 6.0-15kGs; Be preferably 8.0-10.5kGs; And/or
Described material coercivity H b is 1500Oe-3000Oe; Be preferably 1800Oe-2100Oe; And/or
Described material magnetic energy product (BH) m is 5.0-15.0MGOe; Be preferably 9.0-11.5MGOe.
6. the method for making of material as claimed in claim 1, it is characterized in that, described method comprises step:
(1) melting is carried out to the mixture of each component, obtain melting mixture;
(2) described melting mixture is poured in sand mo(u)ld, obtains crystalline orientation alloy, and carry out solution treatment;
(3) the described alloy through solution treatment is placed in magnetic field to cool;
(4) magnetic field Isothermal treatment is carried out to described cooled alloy, obtain described material.
7. method for making as claimed in claim 6, it is characterized in that, described method also comprises:
In melting step: after first high melting point component being melted, add carbon dust and react a period of time, then add low-melting component; And/or
After described casting complete, the alloy obtained is incubated a period of time, then carries out sand removal process after cast.
8. method for making as claimed in claim 6, it is characterized in that, described Isothermal treatment step comprises:
Regulate the temperature of Isothermal treatment environment at 815-830 DEG C; And/or
Control the temperature difference≤± 1 DEG C of Isothermal treatment environment, be preferably≤± 0.5 DEG C; And/or;
The time of described Isothermal treatment is 5-30min, is preferably 10-25min.
9. method as claimed in claim 6, it is characterized in that, described method also comprises:
I () be pre-prepared sand mo(u)ld before described cast step;
(ii) after described Isothermal treatment step, temper is carried out to obtained material.
10. method as claimed in claim 9, it is characterized in that, described temper comprises step:
One-level tempering: be incubated 1-5 hour at 650 DEG C ~ 690 DEG C;
Second annealing: be incubated 6-10 hour at 600 DEG C ~ 640 DEG C;
Three grades of tempering: be incubated 12-24 hour at 550 DEG C ~ 590 DEG C.
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| CN114635070A (en) * | 2022-02-21 | 2022-06-17 | 杭州永磁集团有限公司 | Preparation method of high-toughness alnico magnetic steel |
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